Synthesis · Upgrading Structural Conjugation in Three-Dimensional Ni-Based Metal-Organic Frameworks for Promoting Electrical Conductivity and Specific Capacitance

5 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Partial recipeSource: Main

Route 1: Other

p. 18085 · Experimental Section - Preparation of the Electrode

Metal precursorsNi-BPE positive electrode

Linker precursorsnot applicable; device assembly from preformed electrodes

Solvents3 M KOH aqueous electrolyte

Additivesactivated carbon negative electrode

Atmospherenot reported

Substrate orientationtwo-electrode ASC device

Oxidant / reductantnone reported

Work-upmass ratio adjusted by charge balance q+ = q- according to equation 2

Activationnot reported

Scalability contextDevice assembly described qualitatively; exact electrode masses and separator/packaging not reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-BPE positive electrode	mass balanced by q+ = q-	p. 18085 · Experimental Section - Preparation of the Electrode
Other	activated carbon (AC) negative electrode	mass balanced by q+ = q-	p. 18085 · Experimental Section - Preparation of the Electrode
Electrolyte	KOH aqueous solution	3 M	p. 18085 · Experimental Section - Preparation of the Electrode

Complete recipeSource: Main

Route 2: Hydrothermal

p. 18084 · Experimental Section - Preparation of Ni-BPE

Metal precursorsNi(NO3)2.6H2O (3 mmol, 0.800 g)

Linker precursorsH3BTC (2 mmol, 0.400 g); BPE (2 mmol, 0.400 g)

Solvents50 mL H2O

Additivesnone reported

Atmospherenot reported

Temperature180

Time48

Substrate orientationnot applicable

Oxidant / reductantnone reported

Work-upcooled to room temperature; yellow-green crystals obtained through filtration and drying

Activationnot reported beyond drying

Scalability context100 mL Teflon-lined stainless vessel; yield approximately 70%.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	3 mmol, 0.800 g	p. 18084 · Experimental Section - Preparation of Ni-BPE
Linker	H3BTC (1,3,5-benzenetricarboxylic acid)	2 mmol, 0.400 g	p. 18084 · Experimental Section - Preparation of Ni-BPE
Linker	BPE (1,2-di(4-pyridyl)ethylene)	2 mmol, 0.400 g	p. 18084 · Experimental Section - Preparation of Ni-BPE
Solvent	H2O	50 mL	p. 18084 · Experimental Section - Preparation of Ni-BPE

Complete recipeSource: Main

Route 3: Solvothermal

p. 18084 · Experimental Section - Preparation of Ni-BPY

Metal precursorsNi(NO3)2.6H2O (0.5 mmol, 145 mg)

Linker precursorsH3BTC (0.5 mmol, 0.105 g); BPY (0.5 mmol, 0.079 g)

Solvents10 mL DMF

Additivesnone reported

Atmospherenot reported

Temperature130

Time72

Substrate orientationnot applicable

Oxidant / reductantnone reported

Work-upcooled to room temperature; greenish blue crystals washed with DMF

Activationnot reported

Scalability context23 mL Teflon-lined stainless vessel; method stated to follow previous report but full typical recipe is given.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.5 mmol, 145 mg	p. 18084 · Experimental Section - Preparation of Ni-BPY
Linker	H3BTC (1,3,5-benzenetricarboxylic acid)	0.5 mmol, 0.105 g	p. 18084 · Experimental Section - Preparation of Ni-BPY
Linker	BPY (4,4'-bipyridine)	0.5 mmol, 0.079 g	p. 18084 · Experimental Section - Preparation of Ni-BPY
Solvent	DMF	10 mL	p. 18084 · Experimental Section - Preparation of Ni-BPY

Complete recipeSource: Main

Route 4: Drop Cast

p. 18084 · Experimental Section - Preparation of the Electrode

Metal precursorsas-prepared Ni-BPE

Linker precursorsnot applicable; preformed Ni-BPE framework used

SolventsN-methylpyrrolidone (NMP); acetone, 1 M HCl, and water for Ni foam cleaning

Additivesacetylene black and PVDF binder

Atmospherenot reported

Temperature60

Time24

Substrate orientationNi foam, 1 x 1 cm2 coated from 1 x 2 cm2 cleaned foam

Oxidant / reductantnone reported

Work-upultrasonic cleaning in acetone 10 min, 1 M HCl 30 min, distilled water 10 min; vacuum dried at 60 C; slurry painted, dried at 60 C for 24 h, compressed at 10 MPa for 30 s

Activationelectrode dried at 60 C and compressed; no electrochemical activation reported

Scalability contextLaboratory-scale electrode preparation; mass loading ca. 2 mg.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared Ni-BPE	part of 7:2:1 active:carbon:PVDF mixture	p. 18084 · Experimental Section - Preparation of the Electrode
Additive	acetylene black	part of 7:2:1 mixture	p. 18084 · Experimental Section - Preparation of the Electrode
Additive	polyvinylidene fluoride (PVDF)	part of 7:2:1 mixture	p. 18084 · Experimental Section - Preparation of the Electrode
Solvent	N-methylpyrrolidone (NMP)	appropriate amount	p. 18084 · Experimental Section - Preparation of the Electrode
Other	Ni foam	1 x 2 cm2 cleaned; 1 x 1 cm2 painted	p. 18084 · Experimental Section - Preparation of the Electrode

Complete recipeSource: Main

Route 5: Drop Cast

p. 18084 · Experimental Section - Preparation of the Electrode

Metal precursorsas-prepared Ni-BPY

Linker precursorsnot applicable; preformed Ni-BPY framework used

SolventsN-methylpyrrolidone (NMP); acetone, 1 M HCl, and water for Ni foam cleaning

Additivesacetylene black and PVDF binder

Atmospherenot reported

Temperature60

Time24

Substrate orientationNi foam, 1 x 1 cm2 coated from 1 x 2 cm2 cleaned foam

Oxidant / reductantnone reported

Work-upsame electrode preparation as Ni-BPE; dried at 60 C for 24 h and compressed at 10 MPa for 30 s

Activationelectrode dried at 60 C and compressed; no electrochemical activation reported

Scalability contextLaboratory-scale electrode preparation; mass loading ca. 2 mg.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared Ni-BPY	part of 7:2:1 active:carbon:PVDF mixture	p. 18084 · Experimental Section - Preparation of the Electrode
Additive	acetylene black	part of 7:2:1 mixture	p. 18084 · Experimental Section - Preparation of the Electrode
Additive	polyvinylidene fluoride (PVDF)	part of 7:2:1 mixture	p. 18084 · Experimental Section - Preparation of the Electrode
Solvent	N-methylpyrrolidone (NMP)	appropriate amount	p. 18084 · Experimental Section - Preparation of the Electrode
Other	Ni foam	1 x 2 cm2 cleaned; 1 x 1 cm2 painted	p. 18084 · Experimental Section - Preparation of the Electrode